DE102004010892B3 - Chemically stable solid Li ion conductor of garnet-like crystal structure and high Li ion conductivity useful for batteries, accumulators, supercaps, fuel cells, sensors, windows displays - Google Patents

Chemically stable solid Li ion conductor of garnet-like crystal structure and high Li ion conductivity useful for batteries, accumulators, supercaps, fuel cells, sensors, windows displays

Info

Publication number
DE102004010892B3
DE102004010892B3 DE102004010892A DE102004010892A DE102004010892B3 DE 102004010892 B3 DE102004010892 B3 DE 102004010892B3 DE 102004010892 A DE102004010892 A DE 102004010892A DE 102004010892 A DE102004010892 A DE 102004010892A DE 102004010892 B3 DE102004010892 B3 DE 102004010892B3
Authority
DE
Germany
Prior art keywords
li ion
batteries
garnet
ion conductor
li
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Fee Related
Application number
DE102004010892A
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German (de)
Inventor
Venkataraman Dr. Thangadurai
Werner Prof. Dr. Weppner
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Christian Albrechts Universitaet Kiel
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Christian Albrechts Universitaet Kiel
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Priority to DE102004010892A priority Critical patent/DE102004010892B3/en
Priority claimed from SI200531864T external-priority patent/SI1723080T1/en
Priority claimed from EP14164076.3A external-priority patent/EP2767512B1/en
Application granted granted Critical
Publication of DE102004010892B3 publication Critical patent/DE102004010892B3/en
Application status is Expired - Fee Related legal-status Critical
Anticipated expiration legal-status Critical

Links

Classifications

    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G9/00Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
    • H01G9/004Details
    • H01G9/022Electrolytes, absorbents
    • H01G9/038Electrolytes specially adapted for double-layer capacitors
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G33/00Compounds of niobium
    • C01G33/006Compounds containing, besides niobium, two or more other elements, with the exception of oxygen or hydrogen
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G35/00Compounds of tantalum
    • C01G35/006Compounds containing, besides tantalum, two or more other elements, with the exception of oxygen or hydrogen
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors [EDLCs]; Processes specially adapted for the manufacture thereof or of parts thereof
    • H01G11/54Electrolytes
    • H01G11/56Solid electrolytes, e.g. gels; Additives therein
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00Secondary cells; Manufacture thereof
    • H01M10/05Accumulators with non-aqueous electrolyte
    • H01M10/056Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
    • H01M10/0561Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of inorganic materials only
    • H01M10/0562Solid materials
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M6/00Primary cells; Manufacture thereof
    • H01M6/14Cells with non-aqueous electrolyte
    • H01M6/18Cells with non-aqueous electrolyte with solid electrolyte
    • H01M6/185Cells with non-aqueous electrolyte with solid electrolyte with oxides, hydroxides or oxysalts as solid electrolytes
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M8/00Fuel cells; Manufacture thereof
    • H01M8/10Fuel cells with solid electrolytes
    • H01M8/12Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte
    • H01M8/124Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte characterised by the process of manufacturing or by the material of the electrolyte
    • H01M8/1246Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte characterised by the process of manufacturing or by the material of the electrolyte the electrolyte consisting of oxides
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00Crystal-structural characteristics
    • C01P2002/70Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/77Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by unit-cell parameters, atom positions or structure diagrams
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/40Electric properties
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M2300/00Electrolytes
    • H01M2300/0017Non-aqueous electrolytes
    • H01M2300/0065Solid electrolytes
    • H01M2300/0068Solid electrolytes inorganic
    • H01M2300/0071Oxides
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies or technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10Energy storage
    • Y02E60/13Ultracapacitors, supercapacitors, double-layer capacitors
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies or technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/50Fuel cells
    • Y02E60/52Fuel cells characterised by type or design
    • Y02E60/525Solid Oxide Fuel Cells [SOFC]
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50Manufacturing or production processes characterised by the final manufactured product
    • Y02P70/56Manufacturing of fuel cells

Abstract

Solid lithium ionic conductor with the stoichiometric composition DOLLAR A Li¶6δελλ SrSra Ba Ba¶¶¶ A A (A = Ca, Sr, Ba / B = Nb, Ta) DOLLAR A or DOLLAR A Li¶6¶αa 2¶TaO¶12¶ (A = Sr, Ba).

Description

  • The The invention relates to a chemically stable, solid lithium ion conductor.
  • mobile Energy storage with high energy densities (and high power densities) be for one Variety of technical devices needed especially for Mobile phones and portable computers (e.g., notebooks). Of outstanding Significance are rechargeable chemical energy storage, in particular secondary batteries and supercapacitors.
  • The hitherto highest energy densities in the range of 0.2 to 0.4 Wh / cm 3 are today commercially realized with so-called lithium-ion batteries. These usually consist of a liquid organic solvent (eg EC / DEC) with lithium salt, an anode of graphite with intercalated lithium and a cathode of lithium cobalt oxide, wherein the cobalt may also be partially or completely replaced by nickel or manganese.
  • generally known the lifetime of such lithium ion batteries is quite limited, so they often still while the life of the device to be supplied must be replaced. moreover the replacement is commonly expensive and the disposal of the Old batteries problematic because some of the ingredients are not environmentally friendly.
  • in the Operation, the batteries prove in the prior art in many applications as insufficiently powerful (e.g. Offline operation of a notebook max. for a few hours). For use of electrodes, the higher Allow for tensions for example 5 V or more, the batteries are chemically unstable; the organic electrolyte constituents begin at voltages above 2.5 V to decompose. The liquid Electrolyte is a safety problem anyway: in addition to spill, fire and explosion hazard is also possible the growth of dendrites can lead to high self-discharge and heating.
  • For some technical objectives are liquid electrolyte batteries in principle disadvantageous because they always have to have a minimum thickness and thus as a thin one Energy storage, e.g. on smart cards, are not usable.
  • Also solid lithium ion conductor, such as Li 2.9 PO 3.3 N 0.46 (LIPON) are known and have been used on a laboratory scale in thin film batteries. However, these materials generally have a much lower lithium conductivity than liquid electrolytes. Solid lithium ion conductors with the best ionic conductivities are Li 3 N and Li-β-alumina. Both compounds are very sensitive to water (moisture). Li 3 N already decomposes at a voltage of 0.445 V; Li-β-alumina is not chemically stable.
  • In the work of Thangadurai et al. "Novel almost lithium ion conduction in garnet-type Li 5 La 3 M 2 O 12 (M = Nb, Ta)" (J. Am. Ceram. Soc., 86, 437-440, 2003) was first reported as the garnet for the In particular, the tantalum-containing compound has been shown to have a volume and grain size conductivity in the garnet structure that tends to be on a comparable scale, with total conductivity even exceeding that of Li-β-alumina or Li 9 AlSiO 8 , but still well below the conductivities of LISICON or Li 3 N.
  • It The object of the invention is a solid electrolyte, in particular to provide a solid lithium ion conductor having a high lithium conductivity, a low electronic conductivity and a high chemical stability in terms of lithium activity having.
  • The Task is solved by a solid electrolyte according to claim 1. Give the dependent claims advantageous embodiments.
  • The following Illustrations are for explanation the invention:
  • 1 shows a unit cell of the crystal structure of Li 5 La 3 M 2 O 12 (M = Nb, Ta);
  • 2 shows the measured conductivity of Li 6 BaLa 2 Ta 2 O 12 in comparison with other solid lithium ion conductors.
  • In the already known garnet-type lithium ion conductor according to Thangadurai et al. For example, the NbO 6 and TaO 6 octahedra are surrounded by six Li + ions and two vacancies. In 1 The octahedra are graphically represented together with lanthanum atoms (large spheres) and lithium ions (small spheres). The vacancies can also be occupied by replacing a lanthanum atom per unit cell with an alkaline earth metal, in particular calcium, strontium or barium, and producing lithium excess in the preparation of the material. As a result, a higher lithium conductivity is achieved.
  • The systematic investigation of all materials of the stoichiometry Li 6 ALa 2 B 2 O 12 (A = Ca, Sr, Ba / B = Nb, Ta) shows that especially the tantalum-containing structures have advantageous properties, in particular those with Sr or Ba up A sites.
  • The lithium conductivity of Li 6 ALa 2 Ta 2 O 12 (A = Sr, Ba) is an order of magnitude higher than that of LIPON at 10 -5 S / cm at 20 ° C. The electronic conductivity, however, is negligible. The polycrystalline samples show no large grain boundary resistance, suggesting that charge transport through the bulk determines the resistance. This is another significant difference from many other known solid lithium ion conductors. Since the garnet has a 3D isotropic structure, the lithium line is then also three-dimensional, that is possible without preferential direction.
  • 2 shows the measured conductivity of Li 6 BaLa 2 Ta 2 O 12 in comparison with various previously known solid lithium ion conductors. The material according to the invention has very high ionic conductivities, which can be compared with those of Li 2.5 P 0.5 Si 0.5 O 4 or even Li 3 N.
  • Moreover, Li 6 ALa 2 Ta 2 O 12 (A = Sr, Ba) surprisingly proves to be chemically very stable. In particular, the material shows no discernible changes under heating in contact with molten lithium, which allows to use electrodes even of elemental lithium. At temperatures up to 350 ° C and DC voltages up to 6 V, there are no chemical decompositions, whereby the electrolyte can be used in secondary batteries with voltages above 5 V.
  • Example: Preparation of pellets of Li 6 ALa 2 Ta 2 O 12 (A = Sr, Ba)
  • For the preparation of the samples which form the solid electrolyte, an oxide of the approximate composition Li 6 ALa 2 Ta 2 O 12 (A = Sr, Ba) is required, which is obtained from nitrates, nitrate oxides or lithium hydroxides by grinding and annealing processes. The La 2 O 3 is dried at 900 ° C for twenty-four hours. The weight loss of the lithium during the annealing of the samples is compensated by an excess of 10% of the lithium salt. Sr (NO 3 ) 2 , Ba (NO 3 ) 2 and Ta 2 O 5 may be added, which convert to oxides upon annealing.
  • The Powder is in ball mills with zirconia balls more than twelve Milled in 2-propanol and annealed at 700 ° C for six hours. The Reaction product is at isostatic pressure in pellets or others fittings pressed, at 900 ° C Sintered for twenty-four hours and the samples are taken with it the powder of the same composition covered to excessive losses of Lithium oxide to avoid. The resulting solid electrolyte forms the starting material for Lithium ion batteries.
  • For the preparation of the solid electrolyte samples, it is also possible to use an oxide of the composition Li 6 ALa 2 Ta 2 O 12 (A = Sr, Ba), which has the highest stoichiometric purity (> 99%). This material is also chemically stable to reactions with pure lithium. A 10% weight excess of LiOH.H 2 O is added to compensate for the loss of lithium during the annealing performed as described above. The grinding of the powder is also carried out as above.

Claims (4)

  1. Solid lithium ion conductor, characterized by the stoichiometric composition Li 6 ALa 2 B 2 O 12 , where A = Ca, Sr, Ba and B = Nb, Ta.
  2. A solid lithium ion conductor according to claim 1, characterized by the stoichiometric composition Li 6 ALa 2 Ta 2 O 12 , wherein A = Sr, Ba.
  3. Solid lithium-ion conductor according to claim 1 or 2, characterized by a garnet-like crystal structure.
  4. Solid lithium ion conductor according to one of the preceding Claims, characterized in that it corresponds to lithium activities a voltage of up to 5V elemental lithium is stable.
DE102004010892A 2004-03-06 2004-03-06 Chemically stable solid Li ion conductor of garnet-like crystal structure and high Li ion conductivity useful for batteries, accumulators, supercaps, fuel cells, sensors, windows displays Expired - Fee Related DE102004010892B3 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
DE102004010892A DE102004010892B3 (en) 2004-03-06 2004-03-06 Chemically stable solid Li ion conductor of garnet-like crystal structure and high Li ion conductivity useful for batteries, accumulators, supercaps, fuel cells, sensors, windows displays

Applications Claiming Priority (12)

Application Number Priority Date Filing Date Title
DE102004010892A DE102004010892B3 (en) 2004-03-06 2004-03-06 Chemically stable solid Li ion conductor of garnet-like crystal structure and high Li ion conductivity useful for batteries, accumulators, supercaps, fuel cells, sensors, windows displays
SI200531864T SI1723080T1 (en) 2004-03-06 2005-03-03 Chemically stable solid lithium ion conductors
CN2005800117495A CN101014540B (en) 2004-03-06 2005-03-03 Chemically stable solid lithium ion conductors
JP2007502240A JP5204478B2 (en) 2004-03-06 2005-03-03 Chemically stable solid lithium ion conductor
PCT/EP2005/002255 WO2005085138A1 (en) 2004-03-06 2005-03-03 Chemically stable solid lithium ion conductors
EP05715707.5A EP1723080B1 (en) 2004-03-06 2005-03-03 Chemically stable solid lithium ion conductors
US10/591,714 US7901658B2 (en) 2004-03-06 2005-03-03 Chemically stable solid lithium ion conductor
KR1020067020655A KR101168253B1 (en) 2004-03-06 2005-03-03 Chemically stable solid lithium ion conductors
EP14164076.3A EP2767512B1 (en) 2004-03-06 2005-03-03 Chemically stable solid lithium ion conductors
TW094106655A TWI436949B (en) 2004-03-06 2005-03-04 Chemically stable solid lithium ion conductor
ARP050100838A AR050401A1 (en) 2004-03-06 2005-03-04 Solid ionic conductor, chemically stable
US13/007,773 US8092941B2 (en) 2004-03-06 2011-01-17 Chemically stable solid lithium ion conductor

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DE102004010892B3 true DE102004010892B3 (en) 2005-11-24

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US (2) US7901658B2 (en)
JP (1) JP5204478B2 (en)
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